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Related Concept Videos

2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
¹H NMR: Long-Range Coupling01:27

¹H NMR: Long-Range Coupling

The coupling interactions of nuclei across four or more bonds are usually weak, with J values less than 1 Hz. While these are usually not observed in spectra, the presence of multiple bonds along the coupling pathway can result in observable long-range coupling.
In alkenes, spin information is communicated via σ–π overlap, as seen in allylic (four-bond) and homoallylic (five-bond) couplings. These coupling interactions are stronger when the σ bond is parallel to the alkene π orbitals.
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal and vicinal coupling are observed. For example, consider the COSY spectrum of ethyl acetate, where its 1D proton NMR spectrum is plotted along the vertical and horizontal axes with their corresponding chemical shift scale. Three spots on the diagonal corresponding to the three peaks in the 1D proton spectrum are called diagonal peaks. The COSY...
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse.

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Related Experiment Video

Updated: Jun 20, 2026

Neutron Spin Echo Spectroscopy as a Unique Probe for Lipid Membrane Dynamics and Membrane-Protein Interactions
10:02

Neutron Spin Echo Spectroscopy as a Unique Probe for Lipid Membrane Dynamics and Membrane-Protein Interactions

Published on: May 27, 2021

Efficient solid-state NMR methods for measuring heteronuclear dipolar couplings in unoriented lipid membrane systems.

Sergey V Dvinskikh1, Vasco Castro, Dick Sandström

  • 1Division of Physical Chemistry, Arrhenius Laboratory, Stockholm University, SE-106 91 Stockholm, Sweden.

Physical Chemistry Chemical Physics : PCCP
|October 1, 2009
PubMed
Summary

Two-dimensional solid-state Nuclear Magnetic Resonance (NMR) techniques provide high-resolution proton-carbon (1H-13C) dipolar couplings in unoriented lipid membranes. These advanced NMR methods offer detailed insights into lipid membrane structure and dynamics.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Membrane biophysics and structural biology.

Background:

  • Solid-state NMR is crucial for studying molecular structure and dynamics.
  • Previous methods for determining heteronuclear dipolar couplings under magic-angle spinning (MAS) have been developed.
  • These methods were previously applied to ordered systems like amino acids and columnar liquid crystals.

Purpose of the Study:

  • To demonstrate the effectiveness of two-dimensional (2D) MAS NMR recoupling sequences for analyzing unoriented lipid membranes.
  • To achieve high-resolution proton-carbon (1H-13C) dipolar coupling measurements in lipid bilayers.
  • To validate the applicability of these NMR techniques to complex biological membranes.

Main Methods:

  • Application of two-dimensional (2D) solid-state NMR recoupling sequences.
  • Magic-angle spinning (MAS) to enhance spectral resolution.
  • Measurement of heteronuclear dipolar couplings in hydrated dimyristoylphosphatidylcholine (DMPC) lipid membranes in the liquid-crystalline Lα phase.

Main Results:

  • The 2D MAS NMR sequences yielded unparalleled resolution of 1H-13C dipolar couplings in unoriented lipid membranes.
  • Experimental results obtained from DMPC membranes showed excellent agreement with prior NMR studies.
  • The study confirmed the utility of these techniques for non-crystalline lipid systems.

Conclusions:

  • The employed 2D MAS NMR recoupling methods are highly effective for structural studies of unoriented lipid membranes.
  • These techniques offer a powerful, non-destructive approach to investigate lipid membrane organization and dynamics.
  • The findings support the use of advanced solid-state NMR for characterizing complex biological membrane systems.